Method and apparatus for determining the freezing point of liquids



April 7 1953 J. w. DlcKr-:Y 2,633,736

METHOD AND APPARATUS FOR DETERMINING THE FREEZING POINT oF LIQUTDs Filed March 28. 1949 2 SHEETS-SHEET l IN1/wrok;

BY WITNESS:

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Aprll 7, 1953 J. w. DlcKEY 2,633,736

y METHOD AND APPARATUS FOR DETERMINING THE FREEZING POINT oF LIQUIDS Filed Maron 28, 1949 l z SHEETS- SHEET 2 a5 W96 .95 94 sa WITNESS:

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AT RNEY Patented Apr. 7, 1953 METHOD AND APPARATUS FOR DETERMIN- ING THE FREEZING POINT OF LIQUIDS John W. Dickey, Newiield, N. Y., assgnor to Bendix Aviationl Corporation, a. corporation of Delaware Application March 28, 1949, Serial No. 83,986

The present invention relates to a method and 'apparatus for determining the freezing point of liquids and kmore particularly mixtures of liquids lo 1' .solutions used in the cooling systems'V of internal combustion engines.

It an object of the present invention to provide a novel method of the above type which is simple in operation, accurate in'result. and uniform in determination of the freezing point irrespective of the character of the liquid being iesd- Q It is another object to providesuch a method which, in contra-distinction to methods dependent. on the specific gravity of vthe liquid, .is completely independent of the temperature ci the liquid to bev tested andprovides a direct Vindication without the necessity of any correcting facltors. f ,I t' another object to vprovide such a method inwhich the endpoint is unmistakable, and the indication` thereof may be recorded either manuallyor automatically.

, .'Itis afurther object of the present invention yto provide a novelapparatus for determining the ,freezing points of liquids which is accurate and reliable, and simple in construction and opera- ,.tion.'

Itlis another object to provide such a device which is l'easily portable, requires no powerV con- Qn'ection, and is immediately' available for use ,without the necessity of preparation or adjust- Ln'fient.'..'.

It is' another object to provide such a ljvvhich'furnishesan 'accurate indication oi the freezing'point of the sample irrespective of vari- ,ations in ambient temperature,V the temperature pjffthe sample, or in the skill or ad'eptness of the operator.`

Further objects and advantages Will be apparentffrom the following description taken in con- `negation' with the accompanying drawings which A,illustrate means for carrying out the method, and in which:

Fig. 1 is a vertical, substantially mid-sectional ,yievv of a preferred embodiment of the inven- 1tion; v

'j ff Figli!y is an enlarged detail of the thermometric element and thev surrounding freezing chamber; ".Fig, 3 is a detail of the two-Way valve for controlling the admission and discharge of the sam- ;ple'to befrozen; Y

Fig. 4 is a'secton Fie-13:v i; 'l:'ig`.l 5 "is'a's'ectionftaken Substantially on the l'e--v-S of Fig. 1.`

taken on the line-4 4 of 6 Claims. (CLS- 17) -of the shaft 5 as by means of anchor 2 Fig. 6 is a, side elevation, partly broken away, of a second embodiment of the invention;

Fig. 7 is a section taken substantially on the line 'I-l in Fig. 6; c

Fig. 8 is a sectional detail of a modified form of discharge nozzle with the mounting means therefor; l

Fig; 9 is an enlarged detail in perspective of the means for automatically actuating the arresting mechanism 'for the thermometer needle.. Applicants novel method of determining the freezing point of a liquid comprises briefly, Vthe freezing of a small sample of the'liquid in a thin ,walledchamber in close thermal connection with a thermometric element, applying hydraulic pres'- sure to the sample toeject it from thechamber, Vwarming the chamber and thermometric element till the sample thaws, and obtaining the reading of the thermometer at the instant that the Vsample startsY to emerge from the chamber'. The freezing of the sample may of course be accomplished by any suitable means, but itr has been found possibleY to construct very Vconvenient in'- struments by utilizing for this purpose small tubes of compressed and liquified carbon dioxide which vare commercially available for operatingja'ck's,

inilating tires etc.

It is actually the melting point of the liquid which is determined, but this is, of course, for all practical purposes, the same as the freezing point.

In Fig. 1 of the drawing there is illustrated a pedestal frame I on one inclined side of which there is mounted in a suitable manner a thermometer 2 having a stationary dial 3 anda needle 4 which isfixedly mounted on a shaft 5 journalled in a bearing member 6. 'A tube 'I'of thermally conductive material such as brass' is iixedly mounted on the interior of frame I as by means of a tting 8, and loosely surrounds the shaft 5. As best shown in Fig. 2, the tube 'I is provided with a bearingv member 9 xed therein in any suitable manner and rotatably supporting the rod 5 which extends therethrough. A coiled strip II of thermostatic bi-metal is rigidly attached to the bearing 9 at one end as indicated at I2, and at its other end is xed to the end collar I3.

An outer tube I 4 is mounted co-axially on-the tube 1, the inner diameter of the tube I4 being somewhat larger than the outer diameter of the tube l whereby an annular space or chamber I5 1s provided between the tubes. This space is closed at one end by a sealingpand anchoring means such as a brazed collar I and at the other end the space I5 communicates with the interior of a nipple I1 formed as a reduced extension of the tube I4. The adjacent end of the tube 1 is xedly mounted as shown at I8 on a bearing stud I9 which conforms to the reduced portion 2| of the outer tube I4, and is provided with openings 22 connecting the space I5 between the tubes with the interior of the nipple I1.

Nipple I1 is connected by-avconduit'23 to adiaphragm chamber indicated generally .by `numeral 24 mounted as shown at 25 on the side of the frame I. Chamber 24 'has a iiexible diaphragm 25 suitably mounted therein, and a spring 21 urges the diaphragm to the left in Fig. 1 toward the position there illustrated. Means for flexingthediaphragm to the right in Fig. l so as to dilate the diaphragm is provided inthe form of a link member Y28 fixed as Vindicated at 29 tothe diaphragm and pivotallyconnected at 381to almanually oper- ,able ,cam member 31|, the shape of the cambeing such that when the handle 3 2 thereofv is raised,

the curved portion 33 .will engage theV 'top of .the

diaphragm chamber 2 4 so als to drav/"thelinlr 28v to theright until the flat portion 34 of the cam mem'- ber engages the top of said chamber so as to imvmobilize the cam member.

The other end of the annular .Space 'I5 Vbetween the tubes I4 and 1 'is connected by a nipple' Y35 to a conduit y.36 which is attached to the common connector 31 of ai three-Way valve 38 (Fig. 3,).

'A second connector '39 o f' valve '38 receives one end of a conduit' 4I which terminates at' its other end in an inlet fitting 42 which is preferably provided with a strainer 43. A third connector v44 of ,the valve '33 receives one end of a conduit'll, the opposite end of which is' connected to an outlet fitting 46 which is preferably located over a removable cup 41 forreceiving the discharged liquid.

Asbest shown in Fig. 4, the valve 35 comprises a cap-shaped' rotor 48 having a suitable packing material' such as lrubber seated therein as indicated at 49', said packing member being provided with -an arcuate groove 5I which is adapted to be Ybrought into registry with the lconnectors 31, 39 and -44 of the valve so kas to selectively provide vcommunication between the connector 31 and either the inlet connector 39 or the outlet connector 44 as the rotor is suitably adjusted. The pivotal movement of the rotor is preferably limited iby suitable means ,such as a pin 52 mounted in the stationary body 53 ofthe valve and projecting into an arcuate slot 54 in the rotor.

The outer tube I4 is provided with a series of .circular ns 55 located in spaced relation around the major portion of. its length, and a casing member 56 is arranged to surround and enclose the iins, and is preferably fixedly mounted thereon in any suitable manner as by solder. Alternate iins are flattened off on opposite sides as indicated at 51 so as to provide a tortuous path from one end tothe other of the casing 56. A nipple 58 fixed to the exterior of the casing 56 at an intermediate point and is arranged .to receive tube v55 which extends to a tting indicated generally by numeral 5I mounted on the top of the frame I. VThis fitting comprises a threaded nipple 62 which is adapted to enter the outlet nozzle 630i a standard commercial form of container 64 for liquid carbon dioxide. The iitting 5I also comprises a .pairV of clamp members 55, 66' (Fig. 5) which are vformed -to receive the nozzle 63 andanchor it l:firmly .to the framey I by means of the clamping '.hclts .61, :68. In order to provide a rm support for the carbon dioxide container 64, a cup-shaped receptacle 65 is clamped to the frame I by bolts 1I and 12 which also traverse the clamp members 55, 65. The receptacle 69 is formed to slidably receive the lower end of the container 64,

The carbon dioxide container 54 is Nprovided with the usual valve mechanism indicated generally by numeral 13, whereby when' the container 64 is grasped and rotated in a counterclockwise direction, since the nozzle 63 is held stationary by the clamp "blocks `55,66 the threaded valve 14 will be withdrawn from the seat 'i5 so as to permit .escape of carbon dioxide from the interior of the container throughitube 59 into the interior of the casing 56. .It thereupon traverses the tortuous path provided by the nns 55 and escapesfrom ithe -ends'fof :thecasing 56 after having cooled the casing` by the extraction of heat therefrom'due to the expansion of the carbon dioxide gas. In korder yto restrict the escape of-the gas through the tube '59, a rod '16 is preferably located theremsoras/to provide a `restricted annular 'passagerfor the-gas'. vMeans arepref'erably lprovidedforimmobilv'i'zlng the needle 4 Aof the-thermometer-Zin orderitoi-preserve ,the critical reading thereof. shown 'in Fig. 1, this is accomplished by means cfa Ilexible blade 11 anchored as show-n-'at'13to'the'interior oi lthe thermometer casing and-having' on its ifree end a pad 'I3' of Vsuitable igfrictional materia-Icare ranged toengage a'button'8"Imounted onthefaend of the thermometer shaft 5. Manual means Tor operating "blade 11 is 'provided 'in-ithe'ffcrrn .of a. button rr2 fixed 4to the'v blade at "83 andA mounted on vthe 4thernfioxn'e'ter*case bymeans-of av snap' diaphragm 84 nxed Y'in any suitable-rommel' to said casing. When Athebutton -82 is drawn outwardly, the diaphragm 84 holds Vtheblari'e-IT infretr'acted position as illustrated. When the button 82`-is pushed in, the diaphragm 84" snaps overrits` dead center position and 'presses Athe-*pad "I9 against the button 8I onthe thermometer shaft so as'to prevent rotation of the thermometer :needle In carrying out the process' bymeans ofthe structure described above, 4the-inlet ffittingi hr413 is dropped Yinto 'the liquid to be tested, -the valve 38 is adjusted to' connect the Vinlet vconduit 4I with the conduit 36 leading to the thermometer casing 56, and thecam 3l is raisedso as'to dilate the diaphragm 26 and cause a' sample of the'liquid to 'be drawn through the concluitsand the annular space I5 and into the diaphragm chamber. 'The carbon dioxide container 64 is then rotatedvcolmter-clockwise slightly so as' 'to permit a A small lamount of the iiquied carbon dioxide to escape through the freezing chamber formedby the casing 55. The sample .ofV liquid Within the' annular space YI5V 'is thus immediately frozen. Thecontainer 54 is then closed by clockwise.rotation and theV cam lever 321is released so as to permit the spring 2i to apply .pressure to the diaphragm 126 tending to eject thel trapped iiuid from the diaphragm chamber. Since' the annular space 'I5` is ,at this time filled with frozen fluid, however, `its escape is prevented.

The valve 38' isl thereupon rotatedy toconn'ect the conduit 36 with the outlet conduit 45 andi the outlet fitting 4s is watched to note when .the liquid begins to escapel therefrom. As .the ,ther- 4mometer fitting Warmsup gradually fromthe ambient temperature, the frozen ysample within the space I5 starts to thaw, andthe .pressure of the spring 21 on the diaphragm forces the liquid out of the outlettting .46. As soon as the il'r'st drop appears at the voutletiitting,` theV operator presses the locking button 82'thus'immobillz1ng the thermometer 'needle so as to preserve the readingwhich thus indicates precisely the temperature at which the sample started to' thaw.

It has been found in the use of freeze-point testers as above set forth, that the influx of comparatively warm liquid from the diaphragm chamberinto the freezing space I5 whenl the sample thaws, causesthe thermometer needle to shoot upfrapidly. This provides -averysatisfactory end-point, so that some operators prefer to merely observe the thermometer needle as it slowly rises after the sample-is frozen, and note the reading just before the needle jumps upward. This, of course, renders the immobilization of the thermometer needle unnecessary.

In Figs. 6 to 9 inclusive there is illustrated an embodiment of the invention in which the immobilization of the thermometer needle is brought about automatically.

As shown in Figs. 6 and '1, a thermometer 85 is mounted on the side of a tubular casing 86 whi-ch receives the end of the carbon dioxide container 81. The freezing chamber indicated generally by the numeral 88 is of the same character as that described in the first embodiment, and the freezing operation therein is carried out in the same manner. In this case, however, one end of the freezing chamber is connected by the conduit 89 to a pressure chamber 9| (Fig. 9) which is closed by an elastic diaphragm 92 which is capable of being flexed outwardly When pressure is generated in said chamber. A lever 93 is pivoted at 94 in the thermometer case and is provided at one end with a pad 95 for engaging and immobilizing the rotary mount 99 of the thermometer needle 91. The opposite end of lever 93 rests on the flexible diaphragm 92 whereby when said diaphragm is flexed outwardly it swings the lever 93 to arrest the movement of the thermometer needle. The inlet conduit 98 is connected at one end as indicated at 99 to the pressure chamber 9| and at its other end has an inlet device IUI provided with studs |02 adapted to engage in the bayonet slots III3 of a socket member |04 fixed to the case 86. Socket member |94 has a pad of sealing material |05 such as rubber seated in the bottom thereof so that when the fitting I9| is mounted in the socket, the opening of the fitting is effectively closed.

Freezing chamber 88 is connected by a conduit |06 to the chamber |91 which is formed and operated in the same manner as the chamber 24 described in the first embodiment.

Fig. 8 illustrates an optional method of securing closure of the inlet fitting when it is mounted on the casing 86. As there shown this is accomplished by means of an automatic valve arrangement which is normally held 'open by a compression spring |98 but which is closed as shown at |09 when the fitting is pressed and inserted in the holding clip II I mounted on the casing 8B.

In the operation of this embodiment of the invention the inlet fitting I 0I is placed in the liquid to be tested and the handle II2 of the -cam member is raised in order to compress the bellows spring I I3 and draw a sample of the liquid through the conduit 98, pressure chamber 9 I, conduit 89, freezing chamber 88, conduit |06, and into the diaphragm chamber |01. The inlet fitting |0| is then mounted in the socket member |94, or in the clip I I I as the case may be, so as to close the inlet fitting. The carbon dioxide container 81 is then manipulated as above described to freeze the contents of the chamber 88, after which the cam lever I I2 is released so as to allow 6*. the spring II3 t place pressure lon the frozen sample. The sample is then-simply permitted to thaw, and as soon as thawing starts the pressure oi' the sample is transmitted through the conduit 89 to the pressure chamber 9|, and 'sinceV the conduit 98 is closed at 'the inlet-IUI, this vpressure builds up and exes the diaphragm 92 so asto immobilize the thermometer needle and. thus record the reading of the thermometerat the instant that thawing of the sample started.

Although certain steps of the novel process have been described" in order, and certain physical embodiments of the apparatus used in carrying out the process have been set forth in detail, it will be appreciated that the order of the steps may in some cases be altered to some extent and the precise structure may be varied without departing from the spirit of the invention.

I claim:

1. In a process for determining the thawing point of a liquid the steps of introducing a sample of the liquid into a small chamber which is in thermally conductive relation to the temperature sensitive element of a thermometer, cooling the chamber so as to freeze the sample therein, then terminating the cooling operation, next placing a steady light pressure on the sample in the chamber tending to eject the sample therefrom, then allowing the chamber to warm up by absorption of heat from its surroundings so as to thaw the material therein, and taking the reading of the thermometer at the instant the sample starts to iiow from the chamber under said pressure.

2. In a process as set forth in claim l, the further step of immobilizing the thermometer indicator at the time the sample starts to flow from the chamber under said pressure so as to retain its coincident temperature indication.

3. A freezing point tester for liquids comprising a thermometer having a movable indicating member and a temperature-sensitive element for moving the indicating member, a freezing chamber surrounding the temperature-sensitive element but sealed therefrom and having inlet and outlet openings, a second chamber connected to one of said openings, means for drawing a sample of the liquid to be tested through said freezing chamber and into the second chamber, means for cooling the freezing chamber below the freezing point of said liquid so as to congeal the liquid therein, and means for applying a steady pressure to the liquid in the second chamber, tending to eject the sample therefrom through the freezing chamber.

4. A freezing point tester as set forth in claim 3 including further a conduit receiving the liquid flowing from said freezing chamber when the sample tliaws, means preventing the free flow of the sample from said conduit, and means responsive to hydro-static pressure in said conduit for immobilizing the movable member of the thermometer.

5. A freeze point tester for liquids comprising a thermometer having a temperature sensitive element, a hollow freezing chamber surrounding said element but sealed therefrom having inlet and outlet openings, means for drawing a sample of the liquid to be tested into said chamber comprising a receiver connected to said chamber, a flexible diaphragm closing the receiver, manually operable means for dilating the diaphragm and holding it dilated and elastic means for continuously applying pressure to the diaphragm pxtessurefchamber ttor :mobilizing the .registering mechanism :of tine-thermometer.

AJQHN. EDICKEY.

REFERENCES .CITED The following referencesane fof .record in lthe le -of patent:

Name .Date Horwet..-... Jan. .19.23 .AllemanifehaL Feb., 20 .193.4

Pelich July .12,1933 Edwards. ,A11g. 26,I 19,41 'Webber `.-Sept. '29 .19.42 

